Improved manufacture of deodorized heavy hydrocarbon-oils



. J. MERRILL. MANUFACTURE OF DE ODORIZED HEAVY HYD ROGARBON OIL.

in close, warm rooms,

dilated fittin amt (tjifiinr.

JOSHUA MERRILL, BOSTON, MASSACHUSETTS,

Letters Patent No. 90,284, dated May 18, d

IMPROVED MANUFACTURE OF DEODORIZED HEAVY HYDROCARBON-OILS.

The Schedule referred to in these Letters Patent and making part of the same.

To all whom it may concern.-

Be it known that I, J osnUA MERRILL, of the city of Boston, in the county of Suii'olk, and State of Massacl usetts, have invented a new and improved Manufacture of Deodorized Heavy Hydrocarbon-Oils, suitable for lubricating-oils, or for carriers use; and I do herebydcclare that the following is a full and correct description thereof; and of the mode of manufacture.

My invention relates to the heavy hydrocarbon-oils, which have heretofore been produced bydistilling crude petroleum, or the-crude oils obtained from the distillation of bituminous coals, bituminous shalcs, bituminous schists, asphaltum, and other substances produciug hydrocarbon-oils by distillation.

It has been the practice to treat such heavy oils with acids and alkalies, forthe purpose of removing the disgusting odor peculiar to these oils, which renders them extremely objectionable for use in the arts, and for lubricating-purposes.

Such processes are well known, and improve the character of the odor of the oils; but, nevertheless, the oils so treated have a persistent disagreeablesmell, which makes them ofl"ensive,and undesirable for use as in woollen mauufactories.

Attempts have been made to remove the smell by filtration, with but partial success.

To make heavy hydrocarbi'm-oils free from the characteristic unpleasant odors of heavy hydrocarbon-oils, I take the heavy oils which have been separatcdfi'om the lighter oils, and from mechanical impurities by distillation, and, after chilling and expressing the solid parafline, when such operation is necessary, place them in a still, heated by a fire underneath, and slowly and gradually raise the temperature until from ten to thirty per cent. of the contents of the still are distilled over, when the stillis cooled down and the remaining contents removed.

The matters which go over to the condenser have'a' very foul, offensive, and disgusting odor, but the oil remaining in the still, if'the operation has been properlyconducted, is free from the characteristic ofl'ensive odor of hydrocarbon-cils, and has no smell except a slight odor similar to that of fatty oils.

It can be mixed, in all proportions, with sperm, lard, fish-oils, and vegetable oils, and is character that it takesthe odor of the oil that it is mixed with. If mixed with twenty per cent. of 'spcrmoil, it does notperceptibly change the smell ofthc spermoil.

The process may-be conducted in a common still, heated by fire-heat, as above mentioned, but will be facilitated, and oil of lighter color produced, by introducing superheated steam into the heated oil within the still, as hereinafter more fully described.

When operating by this process upon the parafiine heavy oils obtained from petroleum, bituminous coals, aml shales, and substances producing paraiiinc-oils, I carry on the distillation until the oil which comes from so neutral in its the condenser has a specific gravity of 36 Baums hydrometer, when, if the process be stopped, the remaining oil in the still is inodorous',.or free from empylelllllil-tlfi odors, but, by carrying on the distillation fiirther, andraising the temperature until the oil running from the condenser has a specific gravity of 32 Banm, the remaining-oil will be thicker or more oily, and yet inodorous.

.Vhen operating upon heavy oils, made from asphaltu-m, I continue the distillation until the oil running over from the condenser has a specific gravity of from 28 to 25 Baums hydrometcr.

The temperature within the still will depend upon the character of the oil acted upon, and upon the mode of working the still.

\Vhen superheated steam is used, the temperature is much lower than when the operation is conducted without it, the steam materially assisting in vaporizing the matters that it is desirable to remove.

It is not practicable to specify particularly the specific gravity of the heavy oils used in my new mannfacture. These oils are well known to the trade, and distinguished from the lighter burning-oils and naphthas by the term heavy oils, their specific gravity varying greatly between the asphaltum-oils and parafline-oils.

Heavy hydrocarbon-oils, produced from the same substances, vary considerably in specific gravity, 'by reason of the presence of more or less of the lighter oils, which are always to be found mixed with them, and therefore, the percentage of oil that is to be distilled over in working this process will vary considerably.

I do not assume to know the reason why the abovedescribed process produces heavy oils, free from the characteristic odors of hydrocarbon-oils, but suppose that these odors arise from matters resulting from decomposition at the temperature at which the heavy oils vaporize and go over, and that these matters, after they are condensed with the heavy oils, will vaporize at a temperature lower than that required to vaporize and distil over the heavy oils, and therefore, inay be separated from the heavy oils by distillation in a close still, at a temperature below that required to distil over the heavy oil, which, not being vaporized, will remain freefrom the odorous matters which would result from decomposition at the temperature required to vaporize it and distil it over.

In carrying on my process, I use the heavy hydrocarbon-oils for sale in the market, whether they have been treated by chemicals or not, the result of the process in either case being the same.

The accompanying drawings represent thedistillingapparatus I prefer to use in carrying out my invention--- Figure 1 being a frontelcvation of the still and condenser;

Figure 2, a plan view; and

Figure- 3, :r'vertlcal cross-section of the still and furnace.

Letter 0 represents the still.

I), the tire-place, formed in brick-work, upon which the still is placed, the fire being applied to the bottom of the still.

0, the grate.

d, the ash-pit.

c, the outlet from the fire-place to the chimney.

j, the man-hole, for access to the interior of the still, covered by a suitable man-hole plate.

g, the goose-neck, or pipe, leading from the still to the condenser h.

i, the casing, surrounding the still, provided with doors, jjj, covering apertures in front of the casing,

' and lids, k k k 7;, covering circular apertures in the top of the casing, designed to be opened to admit air to" the body of the still within the casing, in order to regulate the temperature of the still, or to. cool it down rapidly when the fire is'removed from below.

misa small filling-pipe, shown broken'oii' in the drawing, but which should be connected with 'a pump, or a reservoir of oil, and furnished with a shut-ofl cock, to be closed when the still is filled.

So far, the apparatus is substantially-the samev as that described in the Letters Patent of .the United States, granted to me, July 30, 1861.

I will now proceed to describe an apparatus thatl have since invented, for superheating steam, andapplying it to the heated oil within the still, and which may be used with' any still heated by a fire.

I place'a perlectly-tight coil of steam-pipe, n, within the still, at or near the bottom, and connect one v end of the coil with a steam-boiler, by a pipe, n,whichpasses through the ,top of the still, and. is furnished with a cock, hi, to control the admission of steam to the coil. v

Theother end of the coil is connected with air-out- .let-pipe, p, which passes up through the top of'the still.

A stop-cock, p, is placed-near the open end of the outiet-pipe. r v

A return-pipe, r, connected with theoutlet-pipe, between the stop-cock and the still, passes down into the'still, terminating in a horizontal discharge-pipe, a", perforated, as usual, with small holes for the escape of the superheated steam into theoil. The return-pipe r has a stop-cock, 'r", to control t-h passage of the superheated steam from the outlet-pipe,

'through the return-pipe, to within the still, so that, whenit is shut, no superheated steampasses into.

the oil.

The advantage of this arrangement of the superheating-ooil and pipes is, that the steam is superheated iuthe coil to about the temperature of the oil it is to be applied to, by the heat of the oil itself,

and then carried above the top of the still,through the outlet-pipe, in order that the operator may, by turning the cock 1) near the open end of the outletpipe, discharge any water that has got into the coil,

and ascertain \vhen'the steam has become sufficiently superheated before letting it into the ollwithinthe still, through the return-pipe.

7 It is obvious thatthis arrangement of pipes for superheating and discharging superheated steam into the oil, can be used for any operations carried on in stills, which require superheated steam of about the temperature of the contents of the still.

In carrying on my new manufacture of deodorizing heavy oil with this'apparatus, I place the heavy oil to be'deodorized in the still, and heat it by the fire beneath to the required temperature to commence the. operation, the steam being shut oil from the coil, and the outlet-cock being opened, to admit of the expulsion of any water from within the coil.-

When the oil is'dleateii to from about 220 to 300. l ahre' .eits thermometer, depending upon the boiling-points of the oils treated, which vary' greatly, I open the steam-cock carefully, and let steam pass into and through the coil, wherein it becomes rapidly s11 perheatedto about the temperature of the oil.

Having ascertained that the steam passing through the coil is suliicicnlly superheated, 1 close the outletcotk, and then carefully open the cock in the returnpipe, and let. a small amount ot' superheated steam pass down into the still, .where it escapes, by the small openings through the pipe, into the body of the hot oil. I

The superheated steam passes up through the body of the oil, and over to the condenser, carrying along with it the more volatile portionsof the oil, which condense and flow from the condenser intoatank provided for their-reception.

I continue this operation, keeping the fire dull and moderate under the still, and the temperature slowly rising 'all the time, until I distil' ofi' all the volatile distilling oft from twenty to thirty per cent., as-the case may be. I now draw out the'fire, then "shut oil the steam, and leave the oil to cool in the still. is drawn'into suitable tanks, and is ready for, sal and use.

It has been so completely divested of its ,fcetid and pungent odors, having only a slight smell like a fatty oil, and has becomeso oily as to be greatly improved and increased invalueas a lubricating-oil, or'for any purposes itmay be used, either alone or mixed with other oils. 7 v v v v r I prefer to pse superheated steam in working the above described process, because I can work at lower temperature than by the'fire heat alone; but do not with the fire, because I can accomplish the, same re-. sult by fire-heat alone, applied to the stilhiorby any known mode of heating-a still, which will heat the'oil sufiieiently to distil over the. portions of theoil neces- 'sary to be removed; but, in that case, I am obliged to conduct the process at higher temperatures, and

when. superheated steam is used in combination with the fire-heat. l From the above, it will be obvious that my invention consists in producing heavy hydrocarbon-oils, suitable forlubricating and other purposes, and free from the characteristic odors of heavy hydrocarbon-oils,

the volatile matters from which the objectionable odors "arise, and, at the same time, preventing new ffll'l'llar not been separated, so long as they contain heavy oils, because the naphtha and lighter oils will go over first, leaving the heavy oil in the still to be operated upon; and also, because, as-before stated,- the distilled heavy oils always contain more or lessof the lighten bodies, owing to the breaking up of a portionof the-heavy crude oil in the process of distillation I claim---- 7 "The above-described newmanufactureof deodorized heavy hydrocarbon-oils,suitable for lubricating and otherpurposes, free'from the characteristic odors of hydrocarbon-oils, and having a slight smell like fatty oil, tiom heavy hydrocarbon oils, by treating them substantially hereinbet'ore described.

Also, in combination with a still suitable for distilling oils, the superheating-coil, with its steam-pipe, outlet-pipe, and return' -pipe, and their stop-cocks, arranged substantially as described.

Witnesses: I JOSHUA MERRILL.

Guns. H. PLUMPTON, MALooLn-Q. GREENE.

matters, which readily flow out with the steam, usually When cool, it

' wish to confine my invention to its use in combination.

the remaining oil left in the still is darker in color than from heavy,hydrocarbomoils, by distilling from them from which the lighter burning-oils and naphthashave i i i l 

